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13 May.,2024

 

Hypophosphorous acid 50wt. water 6303-21-5

General description

H3PO2, a monobasic oxyacid, is also referred to as phosphinic acid. H3PO2 participates as a reducing agent for the conversion of aromatic and aliphatic diselenides to the corresponding selenols.
It undergoes oxidation in the presence of Ce(IV) and a strong acid to afford cerium(IV) hypophosphite complex ions.

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6303-21-5 | CAS DataBase

[Outline]

Hypophosphorous acid is also known as "hypophosphite" It is colorless oil or deliquescence crystal , it is an important fine chemical product. The main use is as reducing agent for electroless plating, phosphoric prevent discoloration of resins, it can also be used in the esterification reaction catalyst, the refrigerant, in particular for the production of high purity product sodium hypophosphite. There are several methods for preparation, the common industrial method for producing is ion exchange resin method and electrodialysis method.
The chemical properties of hypophosphorous acid, uses, toxicity, and production methods are edited by andy of Chemicalbook. (2016-12-04)[Chemical properties]

It is deliquescent crystals or colorless oil. Melting point: 26.5℃. The relative density (specific gravity): 1.439 (solid, 19℃). It is soluble in water, ethanol and ether, and it can be mixed in any proportion with water, ethanol, acetone. In the air, it easily deliquesce to syrupy liquid, and the aqueous solution is acidic.
Hypophosphorous acid is monobasic acid, in aqueous solution, Hypophosphorous acid is strong acid, Ka = 10-2 (25℃); it is relatively stable at room temperature; disproportionation reaction can proceed at 130℃, decompose into phosphine and phosphorous acid:
2H3PO2=H3PO4+PH3
It has strong reduction, heavy metal salt solution can be restored to metals such as Cu2 +, Hg2 +, Ag +, such as:
4Ag+H3PO2+2H2)=4Ag+H3PO4+4H+
It is weak oxidizer, it can be reduced to phosphine, phosphine when encounters strong reducing agent.[Uses]

1. Hypophosphorous acid is used as reducing agent for electroless plating;
2. It can be used to prevent discoloration of phosphoric acid resin;
3. It is used as esterification catalyst, the refrigerant;
4. It is used to produce hypophosphite, sodium salts, manganese salts, iron salts are generally used as nourishing substances;
5. Hypophosphorous acid is used in medicine and as reducing agent, the determination of arsenic, tellurium and separation of tantalum, niobium and other reagents.
6. It is strong reducing agent, It can be used for the preparation of sodium hypophosphite, calcium phosphate and other hypophosphite.
7. It can be used for the plating bath. Pharmaceuticals. reducing agent. general reagents.
8. It is strong reducing agent, it can be used in making sodium hypophosphite, calcium phosphate and other hypophosphite.
9. This product is widely used as reducing agent, Ag, Cu, Ni, Hg and other metals are reduced to the corresponding metal, for the verification of As, Nb, Ta and other reagents, it can be used for the preparation of Na, K, Ca, Mn, Fe and other types of hypophosphite.[Toxicity]

It is non-combustible. But when contacts with the hole H agent, it will cause fire. When meets oxidizing agent, violent reaction and combustion can proceed. When it is heated to high, it can decompose into highly toxic phosphine gas, or even explode. It is corrosive. Hypophosphorous acid is often added into soft drinks, and because it is not absorbed. So the risk is small, but particularly strong hypophosphite hurt gastrointestinal. Accidentally it splashes into the eyes or contacts skin, plenty of water is used to washed. Production operators should wear protective clothing and other protective clothing. Production equipment should be sealed, workshop should be ventilated well.[HAZARDS IDENTIFICATION]

Hazard statement:
Causes severe skin burns and eye damage.
Causes serious eye damage
Precautionary statements:
Do not breathe dust/fume/gas/mist/vapors/spray.
Wash thoroughly after handling.
Wear protective gloves and eye/face protection.
IF SWALLOWED: Rinse mouth. Do NOT induce vomiting.
IF ON SKIN (or hair): Remove/Take off immediately all contaminated clothing. Rinse skin with water/shower.
IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if
present and easy to do. Continue rinsing.
IF INHALED: Remove victim to fresh air and keep at rest in a position comfortable for breathing.
Immediately call a POISON CENTRE or doctor/physician.
Store locked up.
Dispose of this material and its container to hazardous or special waste collection point.[Preparation method]

1. Phosphorus and barium hydroxide solution is heated,  barium salt Ba (H2PO2) 2 • 2H2O can generate, sulfuric acid is added into hypophosphorous acid barium solution, Ba2+ can precipitate:
Ba(H2PO2)2+H2SO4=BaSO4+2H3PO2
Hypophosphorous acid can be obtained by evaporating under reduced pressure and low temperature crystallization. Due to in this process, the solubility of the barium salt is small, so the concentration of obtained Hypophosphorous acid is not high, industrial product should be purified by recrystallization.
2. the barium oxide (or lime) and solution of white phosphorus is heated together to form secondary barium phosphate (or calcium), and then reacts with sulfuric acid, it is filtered, concentrated to obtain product, or sodium hypophosphite solution proceeds H-type ion exchange resin can derive product. This method requires a large amount of resin, and resin regeneration and washing step is cumbersome, it generally costs more than $ 7 per pound, it is only suitable for small batch production, and not suitable for large-scale industrial applications.
3. Hypophosphorous acid is prepared by electrodialysis method, wherein the electrodialysis cell divides into three parts, they are anode chamber, raw material chamber and cathode chamber, the intermediate is separated by anionic membrane and cationic membrane, between two membranes sodium hypophosphite solution is placed (concentration of 100g/L~500g/L), anode chamber is dilute solution of Hypophosphorous acid 5g/L, anode chamber is dilute sodium hydroxide solution ( 5g /L), between the poles DC (3V~36V) is passed, anode releases oxygen, and generates secondary product of Hypophosphorous acid; cathode emits hydrogen, and generates secondary product of sodium hydroxide, the reaction time is 3~21h. The reactions of anode chamber and cathode chamber are as follows:
anode chamber:
H2O==H++OH-
2OH-==O2+2H2O+4e
H++H2PO2-==H3PO2
cathode chamber:
H2O==H++OH-
2H++2e==H2
Na++OH-==NaOH
Electrodialysis method of preparation Hypophosphorous acid is simple and equipment investment is small, it is suitable for mass production.
4. Starting from the industrial grade sodium hypophosphite, Cl-, SO42-anions which affect the quality indicators of Hypophosphorous acid are removed by precipitation, heavy metal ions are removed from the solution by forming sulfide, and then using strong acid cation exchange resin to obtain sodium secondary phosphate, high purity grade product can obtain. The process can produce high-grade secondary phosphate, technically is feasible, the process is simple, easy operation, good product quality, it can meet the needs of the electronics industry, defense industry and other high-tech fields.

figure 1 Production Process of Hypophosphorous Acid from Industrial Sodium Hypophosphite.
5. Ion exchange resin method: about 70g of cation exchange resin wetted with water is packed into a glass tube with 5 mol/L hydrochloric acid circulating about 15min, after thoroughly washed with water, high purity aqueous sodium hypophosphite aqueous solution (15 g/60 ml H2O) flows through it, the resin column is first washed with 50 ml, then with 25 rnl distilled water. The effluent acid and washing is combined, it is concentrated by evaporation in water bath. The concentrated acid is placed in high vacuum with P205 dryer for dehydration, cooling and crystallization, filtration, recrystallization, to obtain hypophosphorous acid product.[Production method]

Ion exchange resin method: put about 70 g water-soluble cation exchange resins to fill into a glass tube. Circulate with 5 mol/L hydrochloric acid for about 15 min and wash sufficiently with water. Have a high aqueous sodium hypophosphite solution (15 g/60 ml H2O) to flow through the resin column, followed by being washed first with 50 ml water, and then rinsing with 25 rnl distilled water. The effluent acid and the washings were combined and concentrated by evaporation on a water bath. The concentrated acid is send to the highly vacuum, P205 dryer for dehydration, followed by cooling crystallization, filtration and recrystallization to obtain the finished product of hypophosphorous acid.